反应详情

A solution of 4-methoxyaniline (40 g, 0.32 mole) and diethyl ethoxymethylenemalonate (65 mL, 0.32 mole) in Dowtherm A (500 mL) was heated at reflux in a flask fitted with side-arm and condenser, and heating was continued until all the ethanol had distilled off (ca. 0.5 hr). The solution was cooled and pentane was added to give a sticky precipitate. The solvents were decanted off and the residue was treated with more pentane and allowed to stand overnight. The solid was filtered off and washed well with pentane to give the title compound (62.4 g; 78%, contains traces of Dowtherm A).

1. temperatureat reflux in a flask
2. customfitted with side-arm and condenser
3. temperatureheating
4. distillationhad distilled off (ca. 0.5 hr)
5. temperatureThe solution was cooled
6. additionpentane was added
7. customto give a sticky precipitate
8. customThe solvents were decanted off
9. additionthe residue was treated with more pentane
10. filtrationThe solid was filtered off
11. washwashed well with pentane